CN104054744A - Preparation method for suspension seed coating agent employing thiamethoxam and difenoconazole as active ingredients - Google Patents
Preparation method for suspension seed coating agent employing thiamethoxam and difenoconazole as active ingredients Download PDFInfo
- Publication number
- CN104054744A CN104054744A CN201410333230.XA CN201410333230A CN104054744A CN 104054744 A CN104054744 A CN 104054744A CN 201410333230 A CN201410333230 A CN 201410333230A CN 104054744 A CN104054744 A CN 104054744A
- Authority
- CN
- China
- Prior art keywords
- preparation
- agent
- difenoconazole
- coating agent
- suspension seed
- Prior art date
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Links
- 239000011248 coating agent Substances 0.000 title claims abstract description 103
- 239000000725 suspension Substances 0.000 title claims abstract description 101
- 238000002360 preparation method Methods 0.000 title claims abstract description 88
- 239000005760 Difenoconazole Substances 0.000 title claims abstract description 58
- BQYJATMQXGBDHF-UHFFFAOYSA-N difenoconazole Chemical compound O1C(C)COC1(C=1C(=CC(OC=2C=CC(Cl)=CC=2)=CC=1)Cl)CN1N=CN=C1 BQYJATMQXGBDHF-UHFFFAOYSA-N 0.000 title claims abstract description 58
- 239000004480 active ingredient Substances 0.000 title abstract description 8
- 239000005941 Thiamethoxam Substances 0.000 title abstract 4
- NWWZPOKUUAIXIW-FLIBITNWSA-N thiamethoxam Chemical compound [O-][N+](=O)\N=C/1N(C)COCN\1CC1=CN=C(Cl)S1 NWWZPOKUUAIXIW-FLIBITNWSA-N 0.000 title abstract 4
- 238000010008 shearing Methods 0.000 claims abstract description 58
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 55
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 34
- 238000009736 wetting Methods 0.000 claims abstract description 28
- 239000002270 dispersing agent Substances 0.000 claims abstract description 26
- 239000002562 thickening agent Substances 0.000 claims abstract description 20
- 238000001914 filtration Methods 0.000 claims abstract description 18
- 239000002518 antifoaming agent Substances 0.000 claims abstract description 12
- 239000004576 sand Substances 0.000 claims description 101
- NWWZPOKUUAIXIW-DHZHZOJOSA-N (E)-thiamethoxam Chemical compound [O-][N+](=O)/N=C/1N(C)COCN\1CC1=CN=C(Cl)S1 NWWZPOKUUAIXIW-DHZHZOJOSA-N 0.000 claims description 54
- 239000000203 mixture Substances 0.000 claims description 43
- 238000003801 milling Methods 0.000 claims description 36
- -1 through shearing Chemical compound 0.000 claims description 26
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 24
- 238000004040 coloring Methods 0.000 claims description 23
- 230000000361 pesticidal effect Effects 0.000 claims description 21
- 239000000047 product Substances 0.000 claims description 16
- 229920001285 xanthan gum Polymers 0.000 claims description 16
- 238000012163 sequencing technique Methods 0.000 claims description 13
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 claims description 12
- 229920001296 polysiloxane Polymers 0.000 claims description 11
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 claims description 11
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 10
- 229920003171 Poly (ethylene oxide) Polymers 0.000 claims description 10
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 claims description 9
- 239000013530 defoamer Substances 0.000 claims description 9
- 235000014113 dietary fatty acids Nutrition 0.000 claims description 8
- 239000000194 fatty acid Substances 0.000 claims description 8
- 229930195729 fatty acid Natural products 0.000 claims description 8
- 239000000839 emulsion Substances 0.000 claims description 7
- 239000007859 condensation product Substances 0.000 claims description 6
- 150000004665 fatty acids Chemical class 0.000 claims description 6
- PHTQWCKDNZKARW-UHFFFAOYSA-N isoamylol Chemical compound CC(C)CCO PHTQWCKDNZKARW-UHFFFAOYSA-N 0.000 claims description 6
- 229920000151 polyglycol Polymers 0.000 claims description 5
- 239000010695 polyglycol Substances 0.000 claims description 5
- IXPNQXFRVYWDDI-UHFFFAOYSA-N 1-methyl-2,4-dioxo-1,3-diazinane-5-carboximidamide Chemical compound CN1CC(C(N)=N)C(=O)NC1=O IXPNQXFRVYWDDI-UHFFFAOYSA-N 0.000 claims description 4
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 4
- WMGSQTMJHBYJMQ-UHFFFAOYSA-N aluminum;magnesium;silicate Chemical compound [Mg+2].[Al+3].[O-][Si]([O-])([O-])[O-] WMGSQTMJHBYJMQ-UHFFFAOYSA-N 0.000 claims description 4
- 229920001400 block copolymer Polymers 0.000 claims description 4
- 229920001495 poly(sodium acrylate) polymer Polymers 0.000 claims description 4
- 239000011118 polyvinyl acetate Substances 0.000 claims description 4
- 229920002689 polyvinyl acetate Polymers 0.000 claims description 4
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 4
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 4
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 4
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 4
- 239000000661 sodium alginate Substances 0.000 claims description 4
- 235000010413 sodium alginate Nutrition 0.000 claims description 4
- 229940005550 sodium alginate Drugs 0.000 claims description 4
- NNMHYFLPFNGQFZ-UHFFFAOYSA-M sodium polyacrylate Chemical compound [Na+].[O-]C(=O)C=C NNMHYFLPFNGQFZ-UHFFFAOYSA-M 0.000 claims description 4
- STCOOQWBFONSKY-UHFFFAOYSA-N tributyl phosphate Chemical compound CCCCOP(=O)(OCCCC)OCCCC STCOOQWBFONSKY-UHFFFAOYSA-N 0.000 claims description 4
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 claims description 3
- 239000000654 additive Substances 0.000 claims description 3
- QFFVPLLCYGOFPU-UHFFFAOYSA-N barium chromate Chemical compound [Ba+2].[O-][Cr]([O-])(=O)=O QFFVPLLCYGOFPU-UHFFFAOYSA-N 0.000 claims description 3
- 238000009833 condensation Methods 0.000 claims description 3
- 230000005494 condensation Effects 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- 229910021653 sulphate ion Inorganic materials 0.000 claims description 3
- LNAZSHAWQACDHT-XIYTZBAFSA-N (2r,3r,4s,5r,6s)-4,5-dimethoxy-2-(methoxymethyl)-3-[(2s,3r,4s,5r,6r)-3,4,5-trimethoxy-6-(methoxymethyl)oxan-2-yl]oxy-6-[(2r,3r,4s,5r,6r)-4,5,6-trimethoxy-2-(methoxymethyl)oxan-3-yl]oxyoxane Chemical compound CO[C@@H]1[C@@H](OC)[C@H](OC)[C@@H](COC)O[C@H]1O[C@H]1[C@H](OC)[C@@H](OC)[C@H](O[C@H]2[C@@H]([C@@H](OC)[C@H](OC)O[C@@H]2COC)OC)O[C@@H]1COC LNAZSHAWQACDHT-XIYTZBAFSA-N 0.000 claims description 2
- DNIAPMSPPWPWGF-GSVOUGTGSA-N (R)-(-)-Propylene glycol Chemical compound C[C@@H](O)CO DNIAPMSPPWPWGF-GSVOUGTGSA-N 0.000 claims description 2
- BWDBEAQIHAEVLV-UHFFFAOYSA-N 6-methylheptan-1-ol Chemical compound CC(C)CCCCCO BWDBEAQIHAEVLV-UHFFFAOYSA-N 0.000 claims description 2
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 claims description 2
- OTMSDBZUPAUEDD-UHFFFAOYSA-N Ethane Chemical compound CC OTMSDBZUPAUEDD-UHFFFAOYSA-N 0.000 claims description 2
- 229910019142 PO4 Inorganic materials 0.000 claims description 2
- 239000004234 Yellow 2G Substances 0.000 claims description 2
- 230000000996 additive effect Effects 0.000 claims description 2
- 125000002877 alkyl aryl group Chemical group 0.000 claims description 2
- 150000008052 alkyl sulfonates Chemical class 0.000 claims description 2
- 239000000440 bentonite Substances 0.000 claims description 2
- 229910000278 bentonite Inorganic materials 0.000 claims description 2
- SVPXDRXYRYOSEX-UHFFFAOYSA-N bentoquatam Chemical compound O.O=[Si]=O.O=[Al]O[Al]=O SVPXDRXYRYOSEX-UHFFFAOYSA-N 0.000 claims description 2
- 150000001875 compounds Chemical class 0.000 claims description 2
- YRIUSKIDOIARQF-UHFFFAOYSA-N dodecyl benzenesulfonate Chemical compound CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 YRIUSKIDOIARQF-UHFFFAOYSA-N 0.000 claims description 2
- 229940071161 dodecylbenzenesulfonate Drugs 0.000 claims description 2
- 229940083159 ethylene distearamide Drugs 0.000 claims description 2
- GNBHRKFJIUUOQI-UHFFFAOYSA-N fluorescein Chemical compound O1C(=O)C2=CC=CC=C2C21C1=CC=C(O)C=C1OC1=CC(O)=CC=C21 GNBHRKFJIUUOQI-UHFFFAOYSA-N 0.000 claims description 2
- SLGWESQGEUXWJQ-UHFFFAOYSA-N formaldehyde;phenol Chemical compound O=C.OC1=CC=CC=C1 SLGWESQGEUXWJQ-UHFFFAOYSA-N 0.000 claims description 2
- 229920005610 lignin Polymers 0.000 claims description 2
- 229920000609 methyl cellulose Polymers 0.000 claims description 2
- 239000001923 methylcellulose Substances 0.000 claims description 2
- RKISUIUJZGSLEV-UHFFFAOYSA-N n-[2-(octadecanoylamino)ethyl]octadecanamide Chemical compound CCCCCCCCCCCCCCCCCC(=O)NCCNC(=O)CCCCCCCCCCCCCCCCC RKISUIUJZGSLEV-UHFFFAOYSA-N 0.000 claims description 2
- 239000001301 oxygen Substances 0.000 claims description 2
- 229910052760 oxygen Inorganic materials 0.000 claims description 2
- 229920001568 phenolic resin Polymers 0.000 claims description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims description 2
- 239000010452 phosphate Substances 0.000 claims description 2
- 229920002401 polyacrylamide Polymers 0.000 claims description 2
- 229940051841 polyoxyethylene ether Drugs 0.000 claims description 2
- 229920000056 polyoxyethylene ether Polymers 0.000 claims description 2
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 claims description 2
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 claims description 2
- 235000019235 yellow 2G Nutrition 0.000 claims description 2
- 238000000034 method Methods 0.000 abstract description 16
- 239000000575 pesticide Substances 0.000 abstract description 5
- 239000003086 colorant Substances 0.000 abstract 2
- 230000002349 favourable effect Effects 0.000 abstract 1
- 238000000265 homogenisation Methods 0.000 abstract 1
- 238000000227 grinding Methods 0.000 description 44
- 239000002245 particle Substances 0.000 description 40
- 208000019300 CLIPPERS Diseases 0.000 description 21
- 208000021930 chronic lymphocytic inflammation with pontine perivascular enhancement responsive to steroids Diseases 0.000 description 21
- 238000012546 transfer Methods 0.000 description 21
- 230000000694 effects Effects 0.000 description 18
- 238000011282 treatment Methods 0.000 description 18
- 239000011324 bead Substances 0.000 description 15
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 description 15
- 238000012545 processing Methods 0.000 description 15
- 229910001928 zirconium oxide Inorganic materials 0.000 description 15
- 238000011156 evaluation Methods 0.000 description 13
- 238000005338 heat storage Methods 0.000 description 10
- 230000008569 process Effects 0.000 description 10
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- 239000000706 filtrate Substances 0.000 description 7
- 239000000463 material Substances 0.000 description 7
- 238000003756 stirring Methods 0.000 description 7
- QYYMDNHUJFIDDQ-UHFFFAOYSA-N 5-chloro-2-methyl-1,2-thiazol-3-one;2-methyl-1,2-thiazol-3-one Chemical compound CN1SC=CC1=O.CN1SC(Cl)=CC1=O QYYMDNHUJFIDDQ-UHFFFAOYSA-N 0.000 description 6
- 239000003755 preservative agent Substances 0.000 description 6
- 230000002335 preservative effect Effects 0.000 description 6
- 238000003860 storage Methods 0.000 description 6
- 230000035784 germination Effects 0.000 description 5
- 239000002689 soil Substances 0.000 description 5
- 241000238631 Hexapoda Species 0.000 description 4
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 4
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 4
- 241000607479 Yersinia pestis Species 0.000 description 4
- 238000000576 coating method Methods 0.000 description 4
- 201000010099 disease Diseases 0.000 description 4
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- BLJQBTCHXOTSEZ-UHFFFAOYSA-N 2-bromo-3-(4-bromophenyl)-4-hydroxy-6-oxo-7h-thieno[2,3-b]pyridine-5-carbonitrile Chemical compound C1=2C(O)=C(C#N)C(=O)NC=2SC(Br)=C1C1=CC=C(Br)C=C1 BLJQBTCHXOTSEZ-UHFFFAOYSA-N 0.000 description 3
- 241000209140 Triticum Species 0.000 description 3
- 235000021307 Triticum Nutrition 0.000 description 3
- 230000008859 change Effects 0.000 description 3
- 230000006872 improvement Effects 0.000 description 3
- CHHHXKFHOYLYRE-UHFFFAOYSA-M 2,4-Hexadienoic acid, potassium salt (1:1), (2E,4E)- Chemical compound [K+].CC=CC=CC([O-])=O CHHHXKFHOYLYRE-UHFFFAOYSA-M 0.000 description 2
- SVTBMSDMJJWYQN-UHFFFAOYSA-N 2-methylpentane-2,4-diol Chemical compound CC(O)CC(C)(C)O SVTBMSDMJJWYQN-UHFFFAOYSA-N 0.000 description 2
- 235000017060 Arachis glabrata Nutrition 0.000 description 2
- 244000105624 Arachis hypogaea Species 0.000 description 2
- 235000010777 Arachis hypogaea Nutrition 0.000 description 2
- 235000018262 Arachis monticola Nutrition 0.000 description 2
- 229920000742 Cotton Polymers 0.000 description 2
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 2
- 244000299507 Gossypium hirsutum Species 0.000 description 2
- 240000008042 Zea mays Species 0.000 description 2
- 235000005824 Zea mays ssp. parviglumis Nutrition 0.000 description 2
- 235000002017 Zea mays subsp mays Nutrition 0.000 description 2
- 238000002835 absorbance Methods 0.000 description 2
- 239000003905 agrochemical Substances 0.000 description 2
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 description 2
- 229910052921 ammonium sulfate Inorganic materials 0.000 description 2
- 235000011130 ammonium sulphate Nutrition 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- WPYMKLBDIGXBTP-UHFFFAOYSA-N benzoic acid Chemical compound OC(=O)C1=CC=CC=C1 WPYMKLBDIGXBTP-UHFFFAOYSA-N 0.000 description 2
- 239000004202 carbamide Substances 0.000 description 2
- 235000013339 cereals Nutrition 0.000 description 2
- 235000005822 corn Nutrition 0.000 description 2
- 238000000605 extraction Methods 0.000 description 2
- 239000003337 fertilizer Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- LCRMGUFGEDUSOG-UHFFFAOYSA-N naphthalen-1-ylsulfonyloxymethyl naphthalene-1-sulfonate;sodium Chemical compound [Na].C1=CC=C2C(S(=O)(OCOS(=O)(=O)C=3C4=CC=CC=C4C=CC=3)=O)=CC=CC2=C1 LCRMGUFGEDUSOG-UHFFFAOYSA-N 0.000 description 2
- 235000020232 peanut Nutrition 0.000 description 2
- 229920002503 polyoxyethylene-polyoxypropylene Polymers 0.000 description 2
- 235000010241 potassium sorbate Nutrition 0.000 description 2
- 239000004302 potassium sorbate Substances 0.000 description 2
- 229940069338 potassium sorbate Drugs 0.000 description 2
- 238000013441 quality evaluation Methods 0.000 description 2
- 238000012216 screening Methods 0.000 description 2
- WXMKPNITSTVMEF-UHFFFAOYSA-M sodium benzoate Chemical compound [Na+].[O-]C(=O)C1=CC=CC=C1 WXMKPNITSTVMEF-UHFFFAOYSA-M 0.000 description 2
- 239000004299 sodium benzoate Substances 0.000 description 2
- 235000010234 sodium benzoate Nutrition 0.000 description 2
- 239000011780 sodium chloride Substances 0.000 description 2
- 239000007921 spray Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- RNMDNPCBIKJCQP-UHFFFAOYSA-N 5-nonyl-7-oxabicyclo[4.1.0]hepta-1,3,5-trien-2-ol Chemical compound C(CCCCCCCC)C1=C2C(=C(C=C1)O)O2 RNMDNPCBIKJCQP-UHFFFAOYSA-N 0.000 description 1
- 241001136249 Agriotes lineatus Species 0.000 description 1
- 239000005711 Benzoic acid Substances 0.000 description 1
- JISVRKSRAKIYPZ-UHFFFAOYSA-N C=O.C1(=CC=CC2=CC=CC=C12)S(=O)(=O)OCOS(=O)(=O)C1=CC=CC2=CC=CC=C12.[Na] Chemical compound C=O.C1(=CC=CC2=CC=CC=C12)S(=O)(=O)OCOS(=O)(=O)C1=CC=CC2=CC=CC=C12.[Na] JISVRKSRAKIYPZ-UHFFFAOYSA-N 0.000 description 1
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 description 1
- 229920002134 Carboxymethyl cellulose Polymers 0.000 description 1
- 241000289763 Dasygaster padockina Species 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 244000068988 Glycine max Species 0.000 description 1
- 235000010469 Glycine max Nutrition 0.000 description 1
- RCEAADKTGXTDOA-UHFFFAOYSA-N OS(O)(=O)=O.CCCCCCCCCCCC[Na] Chemical group OS(O)(=O)=O.CCCCCCCCCCCC[Na] RCEAADKTGXTDOA-UHFFFAOYSA-N 0.000 description 1
- 239000004698 Polyethylene Substances 0.000 description 1
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 description 1
- 244000046109 Sorghum vulgare var. nervosum Species 0.000 description 1
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- 238000009395 breeding Methods 0.000 description 1
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- YDEXUEFDPVHGHE-GGMCWBHBSA-L disodium;(2r)-3-(2-hydroxy-3-methoxyphenyl)-2-[2-methoxy-4-(3-sulfonatopropyl)phenoxy]propane-1-sulfonate Chemical compound [Na+].[Na+].COC1=CC=CC(C[C@H](CS([O-])(=O)=O)OC=2C(=CC(CCCS([O-])(=O)=O)=CC=2)OC)=C1O YDEXUEFDPVHGHE-GGMCWBHBSA-L 0.000 description 1
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- ULWHHBHJGPPBCO-UHFFFAOYSA-N propane-1,1-diol Chemical class CCC(O)O ULWHHBHJGPPBCO-UHFFFAOYSA-N 0.000 description 1
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- 238000002791 soaking Methods 0.000 description 1
- 229960003885 sodium benzoate Drugs 0.000 description 1
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- 239000004334 sorbic acid Substances 0.000 description 1
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- 239000013638 trimer Substances 0.000 description 1
- RYFMWSXOAZQYPI-UHFFFAOYSA-K trisodium phosphate Chemical compound [Na+].[Na+].[Na+].[O-]P([O-])([O-])=O RYFMWSXOAZQYPI-UHFFFAOYSA-K 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
Landscapes
- Agricultural Chemicals And Associated Chemicals (AREA)
- Pretreatment Of Seeds And Plants (AREA)
Abstract
The invention belongs to the technical field of pesticide preparations, and discloses a preparation method for a suspension seed coating agent employing thiamethoxam and difenoconazole as active ingredients. The preparation method comprises the following steps of adding each component according to a specific sequence, and performing shearing, sanding, homogenization and filtration to obtain the suspension seed coating agent employing thiamethoxam and difenoconazole as the active ingredients, wherein the components comprise a pesticide active ingredient, a wetting dispersant, a film forming agent, a colorant, an antifoaming agent, a thickening agent and water; the specific sequence is water, the wetting dispersant, the colorant and the pesticide active ingredient; the pesticide active ingredient consists of thiamethoxam and difenoconazole. According to the preparation method, the thermal stability of the prepared suspension seed coating agent is remarkably improved, the stability of the suspension seed coating agent is improved, and the method is favorable for the popularization and application of the suspension seed coating agent.
Description
Technical field
The invention belongs to technical field of pesticide preparations, particularly a kind of active component is the preparation method of Diacloden and difenoconazole suspending seed-dressing agent.
Background technology
Soil insect refers to the class pest that the harm phase lives in soil, mainly contains thread clam, crab groove, cutworm and wireworm etc.This class pest is of a great variety, and harm host is wide, as crops such as wheat, corn, Chinese sorghum, cottons.They mainly take food seed, root, stem, piece root, stem tuber, seedling, tender leaf and the growing point etc. of crop, usually cause be short of seedling, disconnected ridge or make growth of seedling bad, very large on crop yield impact.In modern agricultural production, seed chemicals treatment is one of method of the native biography of control soil insect and crops, seed-borne disease economical and convenient.
Seed coating technology is a kind of very universal seed treatment new technology growing up in traditional seed soaking or seed dressing technical foundation.By the seed of dry or moisture state, with the composition such as agricultural chemicals or fertilizer dressing, make outside seed, to form the protective layer with certain function and coated intensity, this process is called seed pelleting, and the material that is wrapped in seed outside is referred to as seed coat agent.Seed coat agent great advantage is to form more firmly film of one deck in seed outside, and in soil, imbibition is not and dissolved for it, and normal required moisture and the air that germinate of permission seed passes through, and the contained material such as agricultural chemicals and seed manure slowly discharges, plays a role.So seed coat agent has the soil insect of killing, seedling stage insect, control sprout term disease and systemic disease, improve percentage of seedgermination, promote seedling healthy growth, reduces the effects such as seed consumption, finally reaches preventing disease pest control, the strong sprout of keeping a full stand of seedings, improves the object of output.
Suspension seed-coating agent is for seed pelleting, has a class preparation of film forming characteristics.Suspension seed-coating agent can make breeding standardization, has again the several functions such as plant protection effect, because it has advantages of that water base property, concentration are high, application safety, the feature of environmental protection is strong and efficiency is high, has been widely used in seed treatment.Suspension seed-coating agent mainly comprises following component: pesticide activity component, wetting dispersing agent, film forming agent, colouring agent, defoamer, thickener, water, but be not limited in these components, can also comprise other additives, as binder, antifreeze, preservative, fertilizer, fertile secondary element etc.
Active component is the suspension seed-coating agent of Diacloden and Difenoconazole, and compared with Diacloden single dose, Difenoconazole single dose, disinsection prophylaxis successful improves, and can be widely used in the seed treatment of the crops such as wheat, corn, soybean, peanut, cotton.But because this formulation is suspension seed-coating agent, suspending agent belongs to thermodynamic unstable system, so the physical stability of product is poor in storing device, be prone to the quality problems such as bleed, thickening and precipitation, cause that system viscosity large fluidity is poor, active ingredient disperses inhomogeneous, lowly or poisoning occurs to pest drug effect, had a strong impact on its production and use.So, be badly in need of a kind of preparation method that active component is the suspension seed-coating agent stability of Diacloden and Difenoconazole that improves.
Summary of the invention
It is the preparation method of Diacloden and difenoconazole suspending seed-dressing agent that goal of the invention of the present invention is to provide a kind of active component.The preparation method of suspension seed-coating agent provided by the invention, having improved active component by specific charging sequence is the heat storage stability of the suspension seed-coating agent of Diacloden and Difenoconazole, gained suspension seed-coating agent stability is high, is more conducive to the promotion and application that active component is the suspension seed-coating agent of Diacloden and Difenoconazole.
In order to realize goal of the invention of the present invention, the present invention adopts following technical scheme:
The invention provides the preparation method that a kind of active component is the suspension seed-coating agent of Diacloden and Difenoconazole, comprising:
Add each component according to specific order, through mixing, shearing, sand milling, homogeneous, filtration, obtain suspension seed-coating agent;
Wherein, component comprises: pesticide activity component, wetting dispersing agent, film forming agent, colouring agent, defoamer, thickener and water;
Specific order is for to add according to the sequencing of water, wetting dispersing agent, colouring agent, pesticide activity component;
This pesticide activity component is made up of Diacloden and Difenoconazole.
Existing active component is that the suspension seed-coating agent preparation method of Diacloden and Difenoconazole does not have strict control to the order of addition of each component, the application finds that the addition sequence of water, wetting dispersing agent, colouring agent, pesticide activity component has a huge impact the stability of gained suspension seed-coating agent in each component of suspension seed-coating agent.Experimental result confirmation, fashionable when adding according to the sequencing of water, wetting dispersing agent, colouring agent, pesticide activity component, contribute to improve the stability that active component is the suspension seed-coating agent of Diacloden and Difenoconazole.And the addition sequence of other components can suitably be adjusted according to process conditions in suspension seed-coating agent.
Heat storage stability test is the test data obtaining by (the being generally 54 DEG C) reservoir of heating, and is used for inferring the stability of the product under storage at normal temperature condition.Because there being a large amount of moisture to exist in suspension seed-coating agent product, and most of Pesticidal products is unstable in water, therefore, and its stability of necessary mensuration.Heat storage stability is whether inspection suspension seed-coating agent formula for a product is reasonable, at a whether stable index request of shelf-life product.Experimental result confirms, the active component that the preparation method that the application provides prepares is that the heat storage stability of the suspension seed-coating agent of Diacloden and Difenoconazole significantly improves, and then improved the stability of this suspension seed-coating agent, be more conducive to the promotion and application that active component is the suspension seed-coating agent of Diacloden and Difenoconazole.
Preferably, preparation method provided by the invention, comprising:
Fetch water, add wetting dispersing agent, mix; Add colouring agent, mix; Add Diacloden, mix; Add Difenoconazole, through shearing, sand milling, homogeneous, filtration, obtain the suspension seed-coating agent that active component is Diacloden and Difenoconazole;
All the other components added before homogeneous.
Preferably, specific sequentially for to add according to the sequencing of water, wetting dispersing agent, colouring agent, pesticide activity component, film forming agent, thickener in preparation method provided by the invention.
In some embodiments of the invention, preparation method provided by the invention comprises:
Fetch water, add wetting dispersing agent, mix; Add colouring agent, mix; Add Diacloden, mix; Add Difenoconazole, after the first shearing, sand milling, add film forming agent, mixing; Add thickener, through the second shearing, homogeneous, filtration, obtain the suspension seed-coating agent that active component is Diacloden and Difenoconazole.
In other embodiment of the present invention, preparation method provided by the invention comprises:
Fetch water, add wetting dispersing agent, mix; Add colouring agent, mix; Add Diacloden, mix; Add Difenoconazole, mix; Add thickener, after the first shearing, sand milling, add film forming agent, through the second shearing, homogeneous, filtration, obtain the suspension seed-coating agent that active component is Diacloden and Difenoconazole.
Preferably, in preparation method provided by the invention, wetting dispersing agent is fatty alcohol-polyoxyethylene ether, alkylphenol polyoxyethylene, polyoxyethylene fatty acid, alkylaryl polyglycol ether, alkylsulfonate, arylsulphonate, alkylnaphthalene sulfonate, fatty acid polyglycol ethylene glycol, dodecyl benzene sulfonate, polyoxyethylene groups phenol formaldehyde condensate, polyoxyethylene poly-oxygen propylene aether block copolymer, alkylnaphthalene sulfonate formaldehyde condensation products, aryl naphthalenesulfonate formaldehyde condensation compound, aliphatic alcohol polyoxyethylene sulfonate, alkylphenol polyoxyethylene sulfonate, lignin and derivative sulfonate thereof, fatty acid ethane additive product phosphate, a kind of or both above mixtures in alkylphenol polyoxyethylene phosphate or alkylphenol polyoxyethylene formaldehyde condensation products sulphate.
More preferably, in preparation method provided by the invention, wetting dispersing agent is lauryl sodium sulfate, dodecyl sodium sulfate, Negel, fatty alcohol polyglycol ether sulphate, fat alcohol polyethylene ether, polyoxyethylene nonylphenol ether, sorbitan fatty acid ester APEO, Fluhyzon formaldehyde condensation products, NNO (sodium methylene bis-naphthalene sulfonate), sodium lignin sulfonate (GY-DM02), calcium lignosulfonate, polycarboxylate (GY-1287), alkyl amine group taurate, sodium methylene bis-naphthalene sulfonate formaldehyde condensation products, polyoxyethylene polyoxypropylene block copolymer Atlox4913, polyoxyethylene polyoxypropylene block copolymer Atlox4894, carboxymethyl cellulose, sodium phosphate trimer, one or more in alkylnaphthalene sulfonate condensation polymer.
Preferably, in preparation method provided by the invention, colouring agent is a kind of or both the above mixtures in Fluorescein red5B, Red-8110, Red-131 or FGR-131, permanent yellow 2G, permanent bordeaux F4R, 3120 sun-proof bright red BBC-1,3117 sun-proof azarin N.
Preferably, in preparation method provided by the invention, film forming agent is a kind of or both the above mixtures in polyvinyl acetate, benzene emulsion, pure-acrylic emulsion, polyvinyl alcohol, polyvinylpyrrolidone, polyacrylamide or Sodium Polyacrylate, E135 (standing grain is large) or KM-m01 (polyesters macromolecule emulsion).
Preferably, in preparation method provided by the invention, thickener is a kind of or both the above mixtures in xanthans, methylcellulose, Sodium Polyacrylate, sodium alginate, polyvinyl alcohol, aluminium-magnesium silicate or bentonite.
Preferably, in preparation method provided by the invention, defoamer is a kind of or both the above mixtures in isooctanol, isoamyl alcohol, tributyl phosphate, ethylenedistearamide, silicone defoaming agent.In some embodiments of the invention, in preparation method provided by the invention, silicone defoaming agent is silicone defoaming agent 32H or silicone defoaming agent 630.
Preferably, in preparation method provided by the invention, the mass ratio of Difenoconazole and Diacloden is 1:1～30.
More preferably, in preparation method provided by the invention, by weight percentage, the content of this pesticide activity component in suspension seed-coating agent is 1%～50%.In some embodiments of the invention, by weight percentage, the content of this pesticide activity component in suspension seed-coating agent is 1%, 34%, 40%, 49.6% or 50%.
Preferably, in preparation method provided by the invention, active component is that the suspension seed-coating agent of Diacloden and Difenoconazole also comprises following component: antifreezing agent and/or preservative.
More preferably, in preparation method provided by the invention, antifreezing agent is a kind of or both the above mixtures in ethylene glycol, propane diols, glycerine, hexylene glycol, urea, ammonium sulfate, sodium chloride or calcium chloride.
More preferably, in preparation method provided by the invention, preservative is a kind of or both above mixtures of benzoic acid, Sodium Benzoate, sorbic acid, potassium sorbate, Kathon CG.
Preferably, in preparation method provided by the invention, by percentage to the quality, the content of wetting dispersing agent in suspension seed-coating agent is 2%～6%.In some embodiments of the invention, by percentage to the quality, the content of wetting dispersing agent in suspension seed-coating agent is 2%, 5% or 6%.
Preferably, in preparation method provided by the invention, by percentage to the quality, the content of film forming agent in suspension seed-coating agent is 2%～5%.In some embodiments of the invention, by percentage to the quality, the content of film forming agent in suspension seed-coating agent is 2%, 3% or 5%.
Preferably, in preparation method provided by the invention, by percentage to the quality, the content of colouring agent in suspension seed-coating agent is 3%～5%.In some embodiments of the invention, by percentage to the quality, the content of colouring agent in suspension seed-coating agent is 3%, 4% or 5%.
Preferably, in preparation method provided by the invention, by percentage to the quality, the content of thickener in suspension seed-coating agent is 0.12%～2.25%.In some embodiments of the invention, by percentage to the quality, the content of thickener in suspension seed-coating agent is 0.12%, 0.15%, 0.5%, 0.65% or 2.25%.
Preferably, in preparation method provided by the invention, by percentage to the quality, the content of defoamer in suspension seed-coating agent is 0.1%～0.5%.In some embodiments of the invention, by percentage to the quality, the content of defoamer in suspension seed-coating agent is 0.1%, 0.2%, 0.3% or 0.5%.
Preferably, in preparation method provided by the invention, by percentage to the quality, the content of preservative in suspension seed-coating agent is 0.1%～0.3%.In some embodiments of the invention, by percentage to the quality, the content of preservative in suspension seed-coating agent is 0.1%, 0.2% or 0.3%.
Preferably, in preparation method provided by the invention, by percentage to the quality, the content of antifreezing agent in suspension seed-coating agent is 3%～5%.In some embodiments of the invention, by percentage to the quality, the content of antifreezing agent in suspension seed-coating agent is 3%, 4% or 5%.
In some embodiments of the invention, in preparation method provided by the invention, when pesticide activity component is made up of Diacloden and Difenoconazole, by percentage to the quality, this suspension seed-coating agent comprises following component: 1%～50% pesticide activity component, 2%～6% wetting dispersing agent, 2%～5% film forming agent, 3%～5% colouring agent, 0.12%～2.25% thickener, 0.1%～0.5% defoamer, 0.1%～0.3% preservative, 3%～5% antifreezing agent, the water of surplus; Wherein the mass ratio of Difenoconazole and Diacloden is 1:1～30.The results show, the particle diameter D (90) of the suspension seed-coating agent containing Diacloden and Difenoconazole preparing according to preparation method provided by the invention is 3 μ m～5 μ m, its heat storage stability significantly improves, compared with control group, significant difference (P < 0.05), other indices have also all obtained improvement to a certain degree, gained suspension seed-coating agent good film-forming property, dressing is even, suspensibility is high, stability is strong, is more conducive to its promotion and application.
In some embodiments of the invention, in preparation method provided by the invention, in the time that thickener is aluminium-magnesium silicate, the addition sequence of thickener for adding before shearing for the first time.In the time that thickener is xanthans, the addition sequence of thickener is after sand milling, before shearing for the second time, adds.
Preferably, in preparation method provided by the invention, first shears instrument used for shearing still.
More preferably, in preparation method provided by the invention, the first shear time is 1h～1.5h.
More preferably, in preparation method provided by the invention, the first rotating speed of shearing is 1000r/m～2000r/m.
More preferably, in preparation method provided by the invention, the second shear time is 1h～1.5h.
More preferably, in preparation method provided by the invention, the second rotating speed of shearing is 1000r/m～2000r/m.
Preferably, in preparation method provided by the invention, sand milling is specially wet method sand milling.
Preferably, in preparation method provided by the invention, sand milling sand milling medium used is zirconium oxide bead.
Preferably, in preparation method provided by the invention, sand milling is specially two step sand millings, through the first sand milling, i.e. and corase grind, then carry out sand milling, i.e. a fine grinding.
More preferably, in preparation method provided by the invention, the particle diameter of the first sand milling sand milling medium used is 0.9mm～1.2mm.
More preferably, in preparation method provided by the invention, the activity coefficient of the first sand milling sand milling medium used is 0.7～0.8.
More preferably, in preparation method provided by the invention, the particle diameter of the second sand milling sand milling medium used is 0.6mm～0.9mm.
More preferably, in preparation method provided by the invention, the activity coefficient of the second sand milling sand milling medium used is 0.7～0.8.
Preferably, in preparation method provided by the invention, sand milling number of times in sand grinding process, sand milling time with sand milling after particle diameter D (90) the < 5 μ m of products therefrom be as the criterion.
Preferably, in preparation method provided by the invention, the aperture of filtering filter screen used is 80 order～100 orders.
The invention provides the preparation method that a kind of active component is the suspension seed-coating agent of Diacloden and Difenoconazole.This preparation method comprises: add each component according to specific order, through shearing, sand milling, homogeneous, filtration, obtain the suspension seed-coating agent that active component is Diacloden and Difenoconazole; Wherein, suspension seed-coating agent comprises following component: pesticide activity component, wetting dispersing agent, film forming agent, colouring agent, defoamer, thickener and water; Specific order is for to add according to the sequencing of water, wetting dispersing agent, colouring agent, pesticide activity component; Pesticide activity component is made up of Diacloden and Difenoconazole.Experimental result confirms, adopts the heat storage stability of the suspension seed-coating agent that preparation method provided by the invention prepares to significantly improve, and has improved the stability of suspension seed-coating agent, is more conducive to the promotion and application of suspension seed-coating agent.
Embodiment
The invention discloses a kind of preparation method of suspension seed-coating agent.Those skilled in the art can be with reference to this paper content, realizes its application, special needs to be pointed out is, and all similar replacements and change apparent to those skilled in the artly, they are all deemed to be included in the present invention.Preparation method of the present invention is described by preferred embodiment, and related personnel obviously can change this paper preparation method in content of the present invention, spirit and scope or suitably change and combination not departing from, and realizes and apply the technology of the present invention.
Preparation method's reagent used and the raw material of a kind of suspension seed-coating agent provided by the invention all can be buied by market.
In order to make those skilled in the art can understand better technical scheme of the present invention, below in conjunction with embodiment, further set forth the present invention:
The preparation of embodiment 1 suspension seed-coating agent
According to following formula, take various supplementary materials:
Preparation method is:
According to water, Atlox4894, GY-DM02, permanent yellow, Diacloden, Difenoconazole, silicone defoaming agent 32H sequencing, join successively to shear in still and (stir while adding, after a upper component mixes, add again next component) shear and mix through high-speed shearing machine, through sand mill wet method sand milling, add afterwards KM-m01, xanthans again, shearing mixes, after uniform filtration, obtain the suspension seed-coating agent containing Diacloden and Difenoconazole.
The preparation of embodiment 2 suspension seed-coating agents
According to following formula, take various supplementary materials:
Preparation method is:
According to the sequencing of water, Atlox4813, Atlox4894, GY-1287, silicone defoaming agent 32H, Kathon CG, 1211-S, Diacloden, Difenoconazole, aluminium-magnesium silicate, ethylene glycol, join successively to shear in still and (stir while adding, after a upper component mixes, add again next component), shear and mix through high-speed shearing machine.The operating parameter of high-speed shearing machine is: clipper model Fu Luke FJS-180X, rotating speed 1470r/m, shear time is 1h.After shearing, transfer in First sand mill, carry out coarse grinding treatment, First sand mill medium sand grinding media is that zirconium oxide bead, particle diameter are 1.2mm, and activity coefficient is 0.7.After coarse grinding treatment completes, transfer in second sand mill and carry out fine grinding processing, second sand mill medium sand grinding media is that zirconium oxide bead, particle diameter are 0.9mm, and activity coefficient is 0.7.In sand grinding process, detect particle diameter by laser particle analyzer and whether reach requirement.After processing through the first sand mill, the second sand mill, the particle diameter D (90) of products therefrom is less than 5 μ m.After sand milling completes, transfer in clipper, add xanthans, E1350, shearing mixes, film forming agent and xanthans can be distributed in suspension seed-coating agent uniformly, the operating parameter of high-speed shearing machine used is: clipper model Fu Luke FJS-180X, rotating speed 1470r/m, shear time is 1h.After shearing, homogeneous, with aperture be 80 object strainer filterings, collect filtrate, obtain the suspension seed-coating agent containing Diacloden and Difenoconazole.
The preparation of embodiment 3 suspension seed-coating agents
According to following formula, take various supplementary materials:
Preparation method is:
According to the sequencing of water, Sodium Benzoate, Atlox4894, GY-1287, permanent bordeaux F4R, silicone defoaming agent 32H, isoamyl alcohol, ethylene glycol, Diacloden, Difenoconazole, join successively to shear in still and (stir while adding, after a upper component mixes, add again next component), shear and mix through high-speed shearing machine.The operating parameter of high-speed shearing machine is: clipper model Fu Luke FJS-180X, rotating speed 1000r/m, shear time is 1.5h.After shearing, transfer in First sand mill, carry out coarse grinding treatment, First sand mill medium sand grinding media is that zirconium oxide bead, particle diameter are 0.9mm, and activity coefficient is 0.8.After coarse grinding treatment completes, transfer in second sand mill and carry out fine grinding processing, second sand mill medium sand grinding media is that zirconium oxide bead, particle diameter are 0.6mm, and activity coefficient is 0.8.In sand grinding process, detect particle diameter by laser particle analyzer and whether reach requirement.After processing through the first sand mill, the second sand mill, the particle diameter D (90) of products therefrom is less than 5 μ m.After sand milling completes, transfer in clipper, add KM-m01, xanthans to shear and mix, film forming agent and xanthans can be distributed in suspension seed-coating agent uniformly, the operating parameter of high-speed shearing machine used is: clipper model Fu Luke FJS-180X, rotating speed 1000r/m, shear time is 1.5h.After shearing, homogeneous, with aperture be 100 object strainer filterings, collect filtrate, obtain the suspension seed-coating agent containing Diacloden and Difenoconazole.
The preparation of embodiment 4 suspension seed-coating agents
According to following formula, take various supplementary materials:
Preparation method is:
According to the sequencing of water, sodium methylene bis-naphthalene sulfonate, tributyl phosphate, 3117 sun-proof azarin N, potassium sorbate, sodium chloride, Difenoconazole, Diacloden, join successively to shear in still and (stir while adding, after a upper component mixes, add again next component), shear and mix through high-speed shearing machine.The operating parameter of high-speed shearing machine is: clipper model Fu Luke FJS-180X, rotating speed 2000r/m, shear time is 1.2h.After shearing, transfer in First sand mill, carry out coarse grinding treatment, First sand mill medium sand grinding media is that zirconium oxide bead, particle diameter are 1 μ m, and activity coefficient is 0.75.After coarse grinding treatment completes, transfer in second sand mill and carry out fine grinding processing, second sand mill medium sand grinding media is that zirconium oxide bead, particle diameter are 0.8mm, and activity coefficient is 0.75.In sand grinding process, detect particle diameter by laser particle analyzer and whether reach requirement.After processing through the first sand mill, the second sand mill, the particle diameter D (90) of products therefrom is less than 5 μ m.After sand milling completes, transfer in clipper, add benzene emulsion, polyvinyl acetate, sodium alginate, shearing mixes, make film forming agent benzene emulsion and polyvinyl acetate, thickener sodium alginate can be distributed in suspension seed-coating agent uniformly, and the operating parameter of high-speed shearing machine used is: clipper model Fu Luke FJS-180X, rotating speed 2000r/m, shear time is 1.2h.After shearing, homogeneous, with aperture be 90 object strainer filterings, collect filtrate, obtain the suspension seed-coating agent containing Diacloden and Difenoconazole.
The preparation of embodiment 5 suspension seed-coating agents
According to following formula, take various supplementary materials:
Preparation method is:
According to water, sorbitan fatty acid ester APEO, tributyl phosphate, urea, ammonium sulfate, 3120 sun-proof bright red, Red-131, Diacloden, Difenoconazole, Kathon CG, bentonitic sequencing, join successively to shear in still and (stir while adding, after a upper component mixes, add again next component), shear and mix through high-speed shearing machine.The operating parameter of high-speed shearing machine is: clipper model Fu Luke FJS-180X, rotating speed 1500r/m, shear time is 1.2h.After shearing, transfer in First sand mill, carry out coarse grinding treatment, First sand mill medium sand grinding media is that zirconium oxide bead, particle diameter are 1mm, and activity coefficient is 0.7.After coarse grinding treatment completes, transfer in second sand mill and carry out fine grinding processing, second sand mill medium sand grinding media is that zirconium oxide bead, particle diameter are 0.8mm, and activity coefficient is 0.7.In sand grinding process, detect particle diameter by laser particle analyzer and whether reach requirement.After processing through the first sand mill, the second sand mill, the particle diameter D (90) of products therefrom is less than 5 μ m.After sand milling completes, transfer in clipper, add polyvinylpyrrolidone, xanthans, shearing mixes, film forming agent polyvinylpyrrolidone and xanthans can be distributed in suspension seed-coating agent uniformly, the operating parameter of high-speed shearing machine used is: clipper model Fu Luke FJS-180X, rotating speed 1500r/m, shear time is 1.2h.After shearing, homogeneous, with aperture be 85 object strainer filterings, collect filtrate, obtain the suspension seed-coating agent containing Diacloden and Difenoconazole.
Embodiment 6 suspension seed-coating agent quality evaluations
Get the suspension seed-coating agent that embodiment 1 to embodiment 5 prepares, investigate the quality of gained suspension seed-coating agent, investigate index and comprise: heat storage stability, cold storage stability, suspensibility, wet screening test, coating uniformity, expulsion rate, germination rate (wheat), germination rate (peanut).The suspension seed-coating agent containing Diacloden and Difenoconazole preparing taking conventional preparation method as a control group 1, other application of sample order prepare containing active component as the suspension seed-coating agent of Diacloden and Difenoconazole as a control group 2, control group 3.
Control group 1 is identical with the formula of Difenoconazole to the Diacloden of control group 3, comprises following various supplementary material:
The preparation method of control group 1 is:
Water intaking, Atlox4813, Atlox4894, GY-1287, ethylene glycol, silicone defoaming agent 32H, Kathon CG, Diacloden, Difenoconazole, 1211-S, join and shear in still, after adding, opens high-speed shearing machine, shears and mix through high-speed shearing machine.The operating parameter of high-speed shearing machine is: clipper model Fu Luke FJS-180X, rotating speed 1000r/m, shear time is 1.5h.After shearing, transfer in First sand mill, carry out coarse grinding treatment, First sand mill medium sand grinding media is that zirconium oxide bead, particle diameter are 0.9mm, and activity coefficient is 0.8.After coarse grinding treatment completes, transfer in second sand mill and carry out fine grinding processing, second sand mill medium sand grinding media is that zirconium oxide bead, particle diameter are 0.6mm, and activity coefficient is 0.8.In sand grinding process, detect particle diameter by laser particle analyzer and whether reach requirement.After processing through the first sand mill, the second sand mill, the particle diameter D (90) of products therefrom is less than 5 μ m.After sand milling completes, transfer in clipper, add KM-m01, xanthans to shear and mix, film forming agent and xanthans can be distributed in suspension seed-coating agent uniformly, the operating parameter of high-speed shearing machine used is: clipper model Fu Luke FJS-180X, rotating speed 1000r/m, shear time is 1.5h.After shearing, homogeneous, with aperture be 100 object strainer filterings, collect filtrate, obtain the suspension seed-coating agent containing Diacloden and Difenoconazole.
The preparation method of control group 2 is:
According to the sequencing of water, Kathon CG, silicone defoaming agent 32H, ethylene glycol, Atlox4813, Atlox4894, GY-1287, Diacloden, Difenoconazole, permanent bordeaux F4R, join successively to shear in still and (stir while adding, after a upper component mixes, add again next component), shear and mix through high-speed shearing machine.The operating parameter of high-speed shearing machine is: clipper model Fu Luke FJS-180X, rotating speed 1000r/m, shear time is 1.5h.After shearing, transfer in First sand mill, carry out coarse grinding treatment, First sand mill medium sand grinding media is that zirconium oxide bead, particle diameter are 0.9mm, and activity coefficient is 0.8.After coarse grinding treatment completes, transfer in second sand mill and carry out fine grinding processing, second sand mill medium sand grinding media is that zirconium oxide bead, particle diameter are 0.6mm, and activity coefficient is 0.8.In sand grinding process, detect particle diameter by laser particle analyzer and whether reach requirement.After processing through the first sand mill, the second sand mill, the particle diameter D (90) of products therefrom is less than 5 μ m.After sand milling completes, transfer in clipper, add KM-m01, xanthans to shear and mix, film forming agent and xanthans can be distributed in suspension seed-coating agent uniformly, the operating parameter of high-speed shearing machine used is: clipper model Fu Luke FJS-180X, rotating speed 1000r/m, shear time is 1.5h.After shearing, homogeneous, with aperture be 100 object strainer filterings, collect filtrate, obtain the suspension seed-coating agent containing Diacloden and Difenoconazole.
The preparation method of control group 3 is:
According to the sequencing of water, Kathon CG, silicone defoaming agent 32H, ethylene glycol, Diacloden, Difenoconazole, permanent bordeaux F4R, Atlox4894, Atlox4813, GY-1287, join successively to shear in still and (stir while adding, after a upper component mixes, add again next component), shear and mix through high-speed shearing machine.The operating parameter of high-speed shearing machine is: clipper model Fu Luke FJS-180X, rotating speed 1000r/m, shear time is 1.5h.After shearing, transfer in First sand mill, carry out coarse grinding treatment, First sand mill medium sand grinding media is that zirconium oxide bead, particle diameter are 0.9mm, and activity coefficient is 0.8.After coarse grinding treatment completes, transfer in second sand mill and carry out fine grinding processing, second sand mill medium sand grinding media is that zirconium oxide bead, particle diameter are 0.6mm, and activity coefficient is 0.8.In sand grinding process, detect particle diameter by laser particle analyzer and whether reach requirement.After processing through the first sand mill, the second sand mill, the particle diameter D (90) of products therefrom is less than 5 μ m.After sand milling completes, transfer in clipper, add KM-m01, xanthans to shear and mix, film forming agent and xanthans can be distributed in suspension seed-coating agent uniformly, the operating parameter of high-speed shearing machine used is: clipper model Fu Luke FJS-180X, rotating speed 1000r/m, shear time is 1.5h.After shearing, homogeneous, with aperture be 100 object strainer filterings, collect filtrate, obtain the suspension seed-coating agent containing Diacloden and Difenoconazole.
(1) assay method of heat storage stability is GB/T19736, is specially:
Evaluation method, for sample is placed in to ampulla bottle, after 54 DEG C of storage 14d, is measured gainer, and evaluation result is in table 1.
(2) assay method of cold storage stability is GB/T19737, is specially:
Sample keeps 1h at 0 DEG C, and observing outward appearance has unchanged.Continue, at 0 DEG C of storage 7d, to test its physical and chemical indexes, evaluation result is in table 1.
(3) assay method of suspensibility is GB/T14825-2006, is specially:
Evaluation method is the suspension that with standard hard water, sample to be tested is mixed with to debita spissitudo, under rated condition, leaves standstill certain hour in graduated cylinder, measures active ingredient mass fraction in 1/10th suspension of bottom, calculates its suspensibility, and evaluation result is in table 1.
(4) assay method of wet screening test is GB/T16150, is specially:
Evaluation method is by the sample weighing up, being placed in beaker soaks, dilutes, fall in the wetting testing sieve of people, directly rinse with mild current from the beginning, then testing sieve is placed in to the basin being filled with water continues washing, residue in sieve is transferred in beaker, dried residue, weigh, calculate fineness, evaluation result is in table 1.
(5) assay method of coating uniformity is the method for describing in 4.9 in NY621-2002, is specially:
Evaluation method is by the capsuled seed of certain grain number, respectively with a certain amount of ethanolic solution extraction, measures the absorbance of extract, calculates sample coating uniformity, and evaluation result is in table 1.
(6) assay method of expulsion rate is the method for describing in 4.10 in NY621-2002, is specially:
Evaluation method is for taking a certain amount of capsuled seed, is placed in the certain hour that vibrates on shaker, by the seed after vibration, with ethanolic solution extraction, measures absorbance, calculates its expulsion rate, and evaluation result is in table 1.
(7) assay method of germination rate is indoor cultivation, is specially:
Evaluation method is by after seed pelleting, be placed between two layers of filter paper, spray certain water gaging and make filter paper wetting, put into plastic packaging bag, 25 DEG C of constant temperature continuous lights are cultivated, all spray certain water gaging every day, keep filter paper moistening, within 7 days, survey germination rate, each processing repeats for 3 times, 100 seeds of each repetition, evaluation result is in table 1.
The quality evaluation result of the suspension seed-coating agent of each group of table 1
From table 1, experimental result is known, contrasts the heat storage stability of each testing sample, and the heat storage stability of the suspension seed-coating agent that embodiment 1 to embodiment 5 prepares is all qualified.And adopt conventional preparation method's control group 1; Application of sample order is the control group 2 of water, wetting dispersing agent, pesticide activity component, colouring agent; Application of sample is sequentially for the suspension seed-coating agent that water, pesticide activity component, colouring agent, the control group 3 of wetting dispersing agent prepare is all defective, illustrate that preparation method provided by the invention has significantly improved the stability of suspension seed-coating agent by specific application of sample order, gained suspension seed-coating agent can steady in a long-term be stored.Other detection indexs that contrast each testing sample are known, the cold storage qualified stability of the suspension seed-coating agent that embodiment 1 to embodiment 5 prepares; Particle size meets the requirements; Expulsion rate meets the requirements; Suspensibility, germination rate all obtain raising to a certain extent.
In sum, embodiment 1 to embodiment 5 prepares suspension seed-coating agent good film-forming property, dressing is even, suspensibility is high, stability is strong.So the preparation method of suspension seed-coating agent provided by the invention can significantly improve the stability of suspension seed-coating agent, be more conducive to the promotion and application of suspension seed-coating agent.
Below be only the preferred embodiment of the present invention, it should be pointed out that above-mentioned preferred embodiment should not be considered as limitation of the present invention, protection scope of the present invention should be as the criterion with claim limited range.For those skilled in the art, without departing from the spirit and scope of the present invention, can also make some improvements and modifications, these improvements and modifications also should be considered as protection scope of the present invention.
Claims (9)
1. active component is a preparation method for the suspension seed-coating agent of Diacloden and Difenoconazole, it is characterized in that, comprising:
Add each component according to specific order, through mixing, shearing, sand milling, homogeneous, filtration, obtain the suspension seed-coating agent that active component is Diacloden and Difenoconazole;
Described component comprises: pesticide activity component, wetting dispersing agent, film forming agent, colouring agent, defoamer, thickener and water;
Described specific order is to add according to the sequencing of described water, described wetting dispersing agent, described colouring agent, described pesticide activity component;
Described pesticide activity component is made up of Diacloden and Difenoconazole.
2. preparation method according to claim 1, is characterized in that, comprising:
Get described water, add described wetting dispersing agent, mix; Add described colouring agent, mix; Add described Diacloden, mix; Add described Difenoconazole, through shearing, sand milling, homogeneous, filtration, obtain the suspension seed-coating agent that active component is Diacloden and Difenoconazole;
Described in all the other, component added before described homogeneous.
3. preparation method according to claim 1, is characterized in that, described specific order is to add according to the sequencing of described water, described wetting dispersing agent, described colouring agent, described pesticide activity component, described film forming agent, described thickener.
4. preparation method according to claim 3, is characterized in that, comprising:
Get described water, add described wetting dispersing agent, mix; Add described colouring agent, mix; Add described Diacloden, mix; Add described Difenoconazole, after the first shearing, sand milling, add described film forming agent, mix; Add described thickener, through the second shearing, homogeneous, filtration, obtain the suspension seed-coating agent that active component is Diacloden and Difenoconazole.
5. preparation method according to claim 1 and 2, it is characterized in that, described wetting dispersing agent is fatty alcohol-polyoxyethylene ether, alkylphenol polyoxyethylene, polyoxyethylene fatty acid, alkylaryl polyglycol ether, alkylsulfonate, arylsulphonate, alkylnaphthalene sulfonate, fatty acid polyglycol ethylene glycol, dodecyl benzene sulfonate, polyoxyethylene groups phenol formaldehyde condensate, polyoxyethylene poly-oxygen propylene aether block copolymer, alkylnaphthalene sulfonate formaldehyde condensation products, aryl naphthalenesulfonate formaldehyde condensation compound, aliphatic alcohol polyoxyethylene sulfonate, alkylphenol polyoxyethylene sulfonate, lignin and derivative sulfonate thereof, fatty acid ethane additive product phosphate, a kind of or both above mixtures in alkylphenol polyoxyethylene phosphate or alkylphenol polyoxyethylene formaldehyde condensation products sulphate.
6. preparation method according to claim 1 and 2, it is characterized in that, described colouring agent is a kind of or both the above mixtures in Fluorescein red5B, Red-8110, Red-131 or FGR-131, permanent yellow 2G, permanent bordeaux F4R, 3120 sun-proof bright red BBC-1,3117 sun-proof azarin N.
7. preparation method according to claim 1 and 2, it is characterized in that, described film forming agent is a kind of or both the above mixtures in polyvinyl acetate, benzene emulsion, pure-acrylic emulsion, polyvinyl alcohol, polyvinylpyrrolidone, polyacrylamide or Sodium Polyacrylate, E135 (standing grain is large) or KM-m01.
8. preparation method according to claim 1 and 2, is characterized in that, described thickener is a kind of or both the above mixtures in xanthans, methylcellulose, Sodium Polyacrylate, sodium alginate, polyvinyl alcohol, aluminium-magnesium silicate or bentonite.
9. preparation method according to claim 1 and 2, is characterized in that, described defoamer is a kind of or both the above mixtures in isooctanol, isoamyl alcohol, tributyl phosphate, ethylenedistearamide, silicone defoaming agent.
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| CN104522045A (en) * | 2014-12-03 | 2015-04-22 | 联保作物科技有限公司 | Pesticide composition, sustained-release pesticidal fertilizer, and preparation methods thereof |
| CN108402037A (en) * | 2018-02-06 | 2018-08-17 | 金华市众鑫农业科技有限公司 | A kind of preparation method for the seed coat agent improving potato bud ratio |
| CN111011376A (en) * | 2019-12-24 | 2020-04-17 | 武威春飞作物科技有限公司 | Corn seed colorful film coating agent and preparation method thereof |
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| CN112823579A (en) * | 2019-11-21 | 2021-05-21 | 沈阳中化农药化工研发有限公司 | Coating component composition of seed treatment agent |
| CN113349211A (en) * | 2021-05-25 | 2021-09-07 | 贵州道元生物技术有限公司 | Compound medicament for preventing and treating plant diseases and insect pests of peanuts, wheat and other plants |
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| CN102308838A (en) * | 2011-09-28 | 2012-01-11 | 联保作物科技有限公司 | Flowable concentrate for seed coating for insecticidal purpose and disease prevention |
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102308838A (en) * | 2011-09-28 | 2012-01-11 | 联保作物科技有限公司 | Flowable concentrate for seed coating for insecticidal purpose and disease prevention |
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| CN104522045A (en) * | 2014-12-03 | 2015-04-22 | 联保作物科技有限公司 | Pesticide composition, sustained-release pesticidal fertilizer, and preparation methods thereof |
| CN108402037A (en) * | 2018-02-06 | 2018-08-17 | 金华市众鑫农业科技有限公司 | A kind of preparation method for the seed coat agent improving potato bud ratio |
| CN112823579A (en) * | 2019-11-21 | 2021-05-21 | 沈阳中化农药化工研发有限公司 | Coating component composition of seed treatment agent |
| CN112823579B (en) * | 2019-11-21 | 2022-05-31 | 沈阳中化农药化工研发有限公司 | Coating component composition of seed treatment agent |
| CN111011376A (en) * | 2019-12-24 | 2020-04-17 | 武威春飞作物科技有限公司 | Corn seed colorful film coating agent and preparation method thereof |
| CN111109296A (en) * | 2020-01-10 | 2020-05-08 | 武威春飞作物科技有限公司 | Colored film coating agent for pumpkin seeds and preparation method |
| CN111184014A (en) * | 2020-01-10 | 2020-05-22 | 武威春飞作物科技有限公司 | Sunflower seed colorful film coating agent and preparation method thereof |
| CN111202086A (en) * | 2020-01-10 | 2020-05-29 | 武威春飞作物科技有限公司 | Colorful film coating agent for shell-free pumpkin seeds and preparation method |
| EP4152929A4 (en) * | 2020-05-18 | 2024-06-05 | UPL Limited | A stabilization system for an agrochemical composition |
| CN113349211A (en) * | 2021-05-25 | 2021-09-07 | 贵州道元生物技术有限公司 | Compound medicament for preventing and treating plant diseases and insect pests of peanuts, wheat and other plants |
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